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Loss on drying (revision 4)

Old revision·08:20, 7 Sep 2024·SigFigSindri

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Loss on drying
AbbreviationLOD
MeasuresTotal volatile mass lost under defined conditions
Contrast withKarl Fischer titration, which measures water specifically
Compendial chapterUSP <731>
Analytical method infobox · conventions

Loss on drying determines the mass a sample loses when heated under defined conditions of temperature, pressure and time. It is simple, requires no specialised reagent, and is widely reported on peptide certificates.[1]

It is not a water determination. The mass lost comprises water and any other volatile component — residual acetonitrile, acetic acid, ammonia from a salt-exchange step — so a loss-on-drying figure is an upper bound on water content rather than a measurement of it. Karl Fischer titration measures water specifically and will generally give a lower number on the same material.[2]

Method

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A weighed sample is dried to constant mass under stated conditions — an oven at a specified temperature, or a desiccator over a specified desiccant, or under vacuum — and the mass difference expressed as a percentage of the starting mass.[1]

The conditions are part of the result. Drying at 105 °C removes more than drying at 60 °C; drying under vacuum removes more than at atmospheric pressure. A figure quoted without its conditions is not comparable with another figure quoted without its conditions.

References

  1. ^ a b United States Pharmacopeia, General Chapter <731>, Loss on Drying.
  2. ^ United States Pharmacopeia, General Chapter <921>, Water Determination.